title: Separation of polychlorinated dibenzo-p-dioxins/furans, non-ortho/mono/di/tri/tetra-ortho-polychlorinated biphenyls, and polybrominated diphenyl ethers groups of compounds prior to their determination with large volume injection gas chromatography-Quadrupole ion storage tandem mass spectrometry.
abstract: Polychlorinated dibenzo-p-dioxins/furans (PCDD/Fs), polychlorinated biphenyls (PCBs) and polybrominated diphenyl ethers (PBDEs) are important environmental contaminants. Their maximum legally allowable levels in food and environment are in the low pg g(-1) range. Therefore some highly selective and sensitive analytical methods must be used to determine them. Prior to final determination by GC/MS the cleaned-up samples have to be split into some fractions in view of large differences in concentrations of various analytes and existence of numerous chromatographic co-elutions (which in any case cannot be fully avoided). The aim of this study was to: (i) develop a robust, time-saving analytical method to isolate, clean-up and fractionate PCBs, PBDEs and PCDD/Fs prior to their determination with gas chromatography/ion trap mass spectrometry; (ii) assess method performance using laboratory validation data and some certified reference materials; (iii) use the developed method to assess PCB/PBDE/PCDD/F levels in samples of commercially available food. A combination of alumina, florisil, modified silica gel and two carbon columns were used for sample cleanup and fractionation. Separate fractions containing dioxins/furans, PBDE, non-ortho, mono-ortho and di-/tri-/tetra-ortho PCBs were obtained. The method statistical parameters were compatible with 1883/2006 EC Regulation (80-120%, RSD below 15%). The method performance was successfully used to evaluation of some real life food samples.
authors.affiliation: Department of Food Analysis, Institute of Agricultural and Food Biotechnology, Rakowiecka 36, 02-532 Warsaw, Poland. Electronic address: roszko@ibprs.pl.
authors.forename: Marek
authors.initials: M
authors.lastname: Roszko
authors.forename: Krystyna
authors.initials: K
authors.lastname: Szymczyk
authors.forename: Renata
authors.initials: R
authors.lastname: Jędrzejczak
mesh_terms: D005591:Chemical Fractionation; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D004147:Dioxins / Q000032:analysis / Q000737:chemistry*; D004784:Environmental Monitoring / Q000379:methods; D004785:Environmental Pollutants / Q000032:analysis / Q000737:chemistry*; D005663:Furans / Q000032:analysis / Q000737:chemistry*; D008401:Gas Chromatography-Mass Spectrometry; D055768:Halogenated Diphenyl Ethers / Q000032:analysis / Q000737:chemistry*; D011078:Polychlorinated Biphenyls / Q000032:analysis / Q000737:chemistry*
chemical_list: D004147:Dioxins; D004785:Environmental Pollutants; D005663:Furans; D055768:Halogenated Diphenyl Ethers; D011078:Polychlorinated Biphenyls
keywords: Carbon column; Dioxins; Fractionation; PBDE